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Engineering Fracture Mechanics 76 (2009) 26662677

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Engineering Fracture Mechanics


journal homepage: www.elsevier.com/locate/engfracmech

A fracture mechanics approach for the prediction of the failure time of polybutene pipes
L. Andena a,*, M. Rink a, R. Frassine a, R. Corrieri b
a b

Dipartimento di Chimica, Materiali e Ingegneria Chimica G. Natta, Politecnico di Milano, Piazza Leonardo da Vinci 32, 20133 Milano, Italy Basell Poliolene Italia, PT&C ARC, G. Natta R&D, P.le P.to Donegani 12, 44100 Ferrara, Italy

a r t i c l e

i n f o

a b s t r a c t
In this work two grades of Isotactic polybutene-1 with a different degree of isotacticity have been investigated; fracture tests have been performed at various temperatures and testing speeds on DCB and SENB samples. Optical methods have been used to record crack advancement. Results of the tests have been interpreted using the fracture mechanics framework; a timetemperature superposition scheme has been adopted to describe crack propagation behaviour over several decades of time-scale. An analytical model has been applied to predict the lifetime of pressurised pipes from experimental fracture data. There is good agreement between model predictions and experimental data obtained from full-scale tests on real pipes. 2009 Elsevier Ltd. All rights reserved.

Article history: Received 31 October 2008 Received in revised form 11 May 2009 Accepted 13 October 2009 Available online 17 October 2009 Keywords: Polybutene Fracture mechanics Timetemperature superposition Pipes

1. Introduction There are several areas in which isotactic polybutene-1 (i-PB1) nds application thanks to its good thermal and mechanical properties: the packaging industry, hot-melt adhesives, tanks for various domestic appliances. In Europe and Asia i-PB1 also became during the past years one of the preferred materials to be used for the manufacturing of hot and cold water plumbing and heating piping systems. i-PB1 offers many advantages in terms of easy, fast installation with a reduced number of joints and connectors compared to much stiffer conventional plumbing materials (such as metals). i-PB1shares with more traditional polyolens good resistance to chemicals and environmental stress cracking in addition to its excellent creep properties even at high temperatures. In the literature there are many works concerning i-PB1s crystallization behaviour (e.g. [1]) and the subsequent transition which occurs between its two crystalline forms (I and II) [2,3]. Fewer works involve its mechanical properties, with widely different approaches. For example, AFM investigation has been used recently to study crazing at the micrometric and nanometric scales [4]. Cohesive zone modelling (CZM), a phenomenological approach which proved to be a powerful method to describe fracture of adhesives and tough polymers [5,6], has been adopted to describe mode I fracture of i-PB1 [7] and different methods have been used to identify cohesive zone parameters. It was shown, however, that i-PB1exhibits a complex fracture behaviour, previously unreported in the literature, with partial instability arising during crack propagation and this limited the effectiveness of CZM in reproducing crack initiation and propagation. Although yielding of i-PB1 has not been extensively studied per se, a better understanding of the damage mechanisms preceding crack initiation could support the investigation of the fracture behaviour of i-PB1.

* Corresponding author. Tel.: +39 0223993207; fax: +39 0270638173. E-mail address: luca.andena@polimi.it (L. Andena). 0013-7944/$ - see front matter 2009 Elsevier Ltd. All rights reserved. doi:10.1016/j.engfracmech.2009.10.002

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Log

ductile failure

brittle failure

Log tf
Fig. 1. Schematic diagram of hoop stress vs. lifetime for a polymeric pressurised pipe.

A key issue in the use of i-PB1 for pressurised pipe applications is the evaluation of their lifetime as related to creep crack growth. This phenomenon consists in the initiation and subsequent slow growth of a crack originating from a surface aw. The materials resistance to this type of fracture is hard to characterise, as the lifetime of pressurised pipes in typical operating conditions may exceed 100 years. Therefore it is common practice to perform accelerated tests at high temperature and extrapolate data to predict pipes lifetime [8]. The schematic diagram shown in Fig. 1 illustrates the outcome of a typical fullscale test on i-PB1 [9]; two distinct regions can usually be recognised. For high hoop stress values (region A), failure occurs due to ductile yielding of the material when the stress in the pipe wall exceeds the yield stress of the material. The term ductile failure is used as large deformations can generally be observed when the pipe cross-section yields before fracture; however, this is not the case for i-PB1 pipes which fail without exhibiting ballooning phenomena, which are quite common in this regime for other polyolens. At lower values of the applied hoop stress (region B) creep crack growth occurs and failures in this region are termed as brittle. This eld is more interesting from the application point of view as pipe failures typically take place under this regime. The main drawback of this kind of test is their long duration (i.e. 12 years) and high cost. Fracture mechanics (FM) can provide an alternative, useful approach. With FM it is possible to characterise fracture properties of a given material from laboratory tests and use them to predict the lifetime of any manufactured article. In [10] FM has been used to study fracture of two grades of i-PB1performing creep tests at high temperature on SENB specimens. The tests lasted for several weeks, thus granting a signicant time saving when compared with full-scale tests on pipes. The authors also developed an analytical model able to predict pipes lifetime and a promising comparison with the reference curves shown in [9] was made. A similar approach has been followed in the present work, performing fracture tests on laboratory specimens. Yet in this study a constant displacement rate rather than a constant load has been applied. This allows a further, signicant reduction in testing times which in this study ranged between a few seconds and a couple of hours these times are much shorter than those required by creep tests, not to speak of full-scale tests on pipes. In addition to that, tests have been carried out with varying speed and temperature in order to ascertain the inuence of these variables on the general fracture behaviour oPB1 and especially on crack stability. Finally, pipe predictions have been obtained using the model developed in [10] and they have been validated against data obtained from full-scale tests. 2. Theoretical background Fracture mechanics data was analysed in terms of the stress intensity factor at the crack tip K for any given crack size a. In the present work only mode I (opening) conditions were considered. Several authors, including Williams [11] and Schapery [12], suggested possible approaches to extend linear elastic FM to viscoelastic materials. Under certain simplifying assumptions, Williams derived the following relationships between the _ stress intensity factor K, the initiation time ti and the crack speed a:

ti B K p _ a A Kq

1 2

in which A, B, p and q are material properties which generally depend on external conditions, such as the temperature. _ Following Schapery [13] it is recognised that a depends on the current value of K but not on its past values and for this reason Eq. (2) applies for any loading history. It becomes thus possible to determine crack propagation parameters from any convenient loading history in a laboratory test and use the obtained data to predict the behaviour of any manufactured item. By combining Eqs. (1) and (2) a prediction of the lifetime tf of a pipe under constant pressure with wall thickness s can be obtained:

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tf ti tp B K p 0

a0

da A Kq

where tp represents the time required for a crack of initial size a0 to propagate across the wall thickness after initiation occurs. Before crack initiation, as the crack size remains constant and equal to a0, the stress intensity factor is also constant and equal to K0. In the present work Eq. (3) has been used, neglecting the initiation time ti in the evaluation of tf. This leads to a conservative prediction of the pipe lifetime. 3. Experimental details The materials investigated are two pipe grades of i-PB1 kindly supplied in the form of pellets by Basell Polyolens. The two grades will be called PB1 and PB2, with PB2 having a higher degree of isotacticity and consequently crystallinity. Fullscale testing run by the producer on pipes made from both materials showed that PB2 offers a better resistance to creep crack growth. The greater degree of crystallinity of PB2 has also been reported to increase elastic modulus and yield stress [10]. The tensile behaviour of i-PB1 is characterised by the absence of strain localisation and necking. The pellets were compression moulded into 170 120 10 mm plates. After cooling from the melt, i-PB1 crystallizes in form II, which is characterised by tetragonal symmetry. This form is unstable at room temperature and spontaneously evolves into form I, which has an hexagonal lattice. To allow for completion of the transition, specimens were cut and machined at least 15 days after moulding [10], and then tested. Fracture experiments under pure mode I conditions have been run on double cantilever beam (DCB) and single edge notch bending (SENB) samples, shown in Fig. 2. Relevant dimensions are listed in Table 1. SENB conguration was used only on preliminary tests on PB2, before moving onto DCB which grants a more stable crack propagation. Also, the longer ligament of DCB specimens grants the acquisition of more data and extended fracture surfaces (see Table 1). Notches in the case of SENB were made by means of razor sliding. The same apparatus could not be used for DCB, due to the larger dimensions: the samples were rst cut using a saw and then a razor blade was pushed into the material. On both congurations the nal root radius of the notches was about 13 lm. The use of two different notching techniques can induce a different degree of damage in the area surrounding the notch tip. This may in turn lead to a different behaviour at crack initiation; however this is not very important for this study in which only crack propagation has been considered.

W a B Bn

P
2h

P
2h

P
W a

Bn B

Fig. 2. DCB (above) and SENB (below) samples used for the fracture tests.

L. Andena et al. / Engineering Fracture Mechanics 76 (2009) 26662677 Table 1 Nominal dimensions of DCB and SENB samples. DCB 2h W a B Bn 45 mm 150 mm 4575 mm 10 mm 6 mm 60 8 mm SENB 2h W a B Bn

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a
U

80 mm 20 mm 10 mm 10 mm 8 mm 60

Table 2 Parameters of the pipe model. s R0 a0 e 2 mm 22 mm 50 lm 1

Side grooves were also introduced in order to guide crack advancement along the notch plane. Great care was taken during specimen preparation in order to ensure proper alignment of notch and grooves. Tests were performed on an Instron 1185R5800 screw-driven electro-mechanical dynamometer tted with an environmental chamber. Constant crosshead speeds of 1, 10 and 100 mm/min were used for the tests run at temperatures of 23 C, 50 C, 70 C and 90 C For every testing condition (sample geometry, speed, temperature) at least two specimens were tested. Crack advancement was monitored using a photo-camera (at 1 mm/min) or a video-camera (at 10 and 100 mm/min) with a calibration gauge applied on the specimens. ImageJ software was used to process the captured images. 4. Evaluation of the stress intensity factors The stress intensity factor K has been evaluated for both testing congurations from the measurements of load and crack length recorded during the tests. In the case of SENB specimens the widely known formula:

K f a=W

P B W 0:5

has been used, in which f(a/W) is a non-dimensional shape factor [14]. For the DCB conguration the formula:

p P a K2 3 1:5 Bh

is generally used. However, Eq. (5) works well only for a/h > 70, which is not the case for the samples tested in the present study. This has been discussed in [15] where an alternative formula by Kanninen is proposed, in which the accuracy of the simple beam theory is improved using EulerBernoulli beam theory together with a Winkler foundation. The resulting equation applies for a/h > 2:

 p P a  h K2 3 1 0:64 1:5 a Bh

These expressions are derived according to linear elastic fracture mechanics (LEFM). To ensure validity of LEFM, small scale yielding and plane strain conditions should be fullled. This can be guaranteed if the specimens meet appropriate size criteria: the size of the plastic zone around the crack tip shall be signicantly smaller than the specimen dimensions, i.e. the thickness B, the crack length a and the ligament length (Wa). The characteristic length of the plastic zone, rp, can be estimated from the following equation [15]:

 rp

KC

2 7

rY

in which KC and rY are the material fracture toughness and yield stress respectively. For both i-PB1 grades rp is approximately 8 mm [7], a value which is comparable with the specimen thickness. However, the inuence of thickness on the fracture properties of PB1 and PB2 has already been investigated on SENB samples in [16] and no effect has been reported in the range between 5 and 20 mm. An effect of the ligament width has been observed instead, with a decrease of the toughness for small values of (Wa); this was already reported by Hashemi and Williams in [17] and it can be explained considering the constraint that such a small ligament size exerts on the plastic zone which, as a consequence, is not free to fully develop.

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Nevertheless in the present study the ligament size was always very large compared with the values below which this effect can be observed. A further evidence of the validity of the LEFM approach is that DCB and SENB K vs. da/dt data at the same temperature are consistent with each other. In the same way, values of critical KC determined according to LEFM at crack initiation on CT and SENB specimens were found to be equal in [7]. The independence of K from the loading conguration proves that it is an adequate parameter for studying the fracture behaviour of i-PB1. 5. Results As previously reported for i-PB1 in [7], partially unstable crack propagation has been observed on both DCB and SENB samples, with instability randomly occurring amidst stable propagation. As the crack begins to propagate a small whitened region forms ahead of the crack tip. The fracture advances through a continuous tearing of this region until for some reason crack propagation stops at the centre of the specimen cross-section. This zone becomes highly stretched until an instability ensues, with the crack jumping ahead on the whole crack front, and a signicant load drop is recorded (see Fig. 3). The amount of the load drop is proportional to the sudden crack advancement. Stable propagation then immediately resumes. These processes take place in a small region localised ahead of the crack tip while the material outside this process zone is largely unaffected by crack propagation, i.e. there is no sign of large scale ductility or necking. The two fracture mechanisms (i.e. stable and unstable propagation) are characterised by a different appearance of the relevant fracture surfaces. Stable propagation originates a rough surface lighter than the original polymer colour due to some whitening which is associated to a very limited degree of ductility. On the other hand regions affected by instabilities are darker than the original polymer and almost at; their size depends on the extent of the crack jumps. The general fracture behaviour of both materials as well as the occurrence of instabilities was seen to be independent of the testing conguration but it is strongly affected by variables such as the testing speed and the temperature. Figs. 46 show fracture surfaces of PB1 and PB2 DCB samples tested at 1, 10 and 100 mm/min and 23, 50 and 70 C. Data at 50 C and to a minor extent at 23 C show that an increase in the testing speed favours unstable propagation, as the dark zones are larger and present in greater numbers. This is not observed at 70 C, temperature at which propagation is stable for all testing speeds; at these temperature the fracture surface becomes very rough, with a central ridge which can also be observed at 50 C, 1 mm/min. While above room temperature areas of stable and unstable propagation can be easily identied, at 23 C it is harder to distinguish between them as the regions interested by the two mechanisms are small and intimately mixed. No signicant differences have been observed in the fracture phenomenology of PB1 and PB2. To nd a correlation between the stress intensity factor and the crack speed, K values have been determined using Eqs. (4) and (6). The crack speed, da/dt, could be easily obtained by direct numerical differentiation of crack length vs. time data.

350 300 250 Load Crack length

140 130 120

Crack length (mm)

110 100 90

Load (N)

200 150 100 50 0

80 70 60 50 40

10

20 30 40 Displacement (mm)

50

60

Fig. 3. Load and crack length vs. displacement curves of a PB1 DCB sample tested at 50 C and 10 mm/min. The correlation between load drops, crack jumps and dark zones on the fracture surface is evident; the bright surface is originated by stable crack propagation.

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Fig. 4. Fracture surfaces of PB1 and PB2 samples tested at 1, 10 and 100 mm/min and 23 C.

Fig. 5. Fracture surfaces of PB1 and PB2 samples tested at 1, 10 and 100 mm/min and 50 C.

However the presence of frequent and/or large crack jumps limits the usefulness of this approach. Yet even when instabilities occur there are large load drops but K values remain almost constant because a increases (see Fig. 7). Moreover, the combination of stable and unstable crack propagation gives rise to an average crack speed which can be determined by a linear t of crack length vs. time data. The average K and da/dt values are reproducible within tests performed in the same conditions (temperature and speed) and they have been used in the following analysis, as they are believed to truly represent the materials behaviour. However, this approach has the obvious drawback of generating only a single data point for each test. Figs. 8 and 9 show K vs. da/dt data at the various temperatures for PB1 and PB2 respectively. According to Eq. (2), K vs. da/ dt curves are expected to be straight lines on a bilogarithmic scale. It is hard to detect a single slope of the data for all temperatures. Moreover, data at 50 C do not fall on straight line.

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Fig. 6. Fracture surfaces of PB1 and PB2 samples tested at 1, 10 and 100 mm/min and 70 C.

3.0 2.5 2.0 1.5 1.0 0.5

PB2
K Crack length

23C

1mm/min

140 130 120

Crack length(mm)

110

K (MPa*m1/2 )

avg K 100
90 80 70 60

avg da/dt
0.0 0

50

40 600 1200 1800 2400 3000 3600 4200 4800 5400

Time (s)
Fig. 7. Typical K and crack length vs. time curves for two DCB samples having different initial crack lengths of 45 and 75 mm; dashed lines indicate the average values of K and da/dt determined during the analysis.

Data at different temperatures can be interpreted using timetemperature superposition, a reduction scheme which is widely accepted in the literature concerning polymers. An example of its application to K vs. da/dt fracture data can be found in [18,19]. Basically one temperature is selected as a reference temperature; data points belonging to another temperature are shifted along the crack speed axis until they superimpose with the reference curve. The process is repeated for the next  temperature and so on, until all data merge on a single master curve at the reference factor. The time shift factor a23 C T T required for each temperature is usually reported on an Arrhenius plot as a function on the reciprocal of temperature and the slope of this plot can be related to the activation energy of the mechanical process involved. This scheme was applied to PB1 and PB2 data in Figs. 8 and 9 and a K vs. da/dt master curve at 23 C was obtained for both  materials, as shown in Fig. 10. The shift factor a23 C T was found to be the same: this quantity seems to be independent of T the materials crystallinity. A similar result was found in [10] for the shift factor related to relaxation modulus and yield  stress. Values of a23 C T are reported on an Arrhenius plot in Fig. 11, where a linear dependence on the reciprocal of temT perature can be observed. In Fig. 10 a knee is clearly visible between crack speeds of about 103 to 102 mm/s, indicating a transition between two regions with a different slope in the K vs. da/dt curve. Data analysis reveals that the two regions are

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0.40 0.35 0.30 0.25 DCB23C DCB50C DCB70C

PB1

logK (MPam )

0.20 0.15 0.10 0.05 0.00 -0.05 -0.10


-5 -4 -3 -2 -1 0 1

log da/dt (mm/s)


Fig. 8. K vs. da/dt data at 1, 10 and 100 mm/min for PB1.

0.40 0.35 0.30 0.25 DCB23C DCB50C DCB70C SENB50C SENB70C SENB90C

PB2

log K(MPam)

0.20 0.15 0.10 0.05 0.00 -0.05 -0.10 -5 -4 -3 -2 -1 0 1

log da/dt (mm/s)


Fig. 9. K vs. da/dt data at 1, 10 and 100 mm/min for PB2.

0.35 0.30 0.25 stable crack propagation

logK (MPam)

0.20 0.15 0.10 0.05 0.00 -0.05 -5 -4 -3 -2 -1 0 1 PB1 PB2 partially unstable crack propagation

log da/dt (mm/s)


Fig. 10. K vs. da/dt master curves for PB1 and PB2 at 23 C. Dashed lines represent the slopes for the stable and partially unstable regimes.

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Fig. 11. Shift factor of K vs. da/dt curves as a function of temperature for both materials studied.

characterised by a distinct behaviour: for K values below the knee stable crack propagation is observed while the values above are associated to partially unstable propagation. In the latter region the crack speed is much more sensitive to the applied K, i.e. an increase of K will cause an increase of da/dt which is larger than in the case of purely stable propagation. It is found then that the simple power-law model detailed in Section 2 can be used to describe propagation data for a given mechanism but the transition between the two mechanisms needs to be correctly taken into account according to the effective K range for a given application. Direct comparison of the two master curves clearly shows that crack propagation on PB1 is faster than PB2 for any level of applied K. This result is in good agreement with results of full-scale testing on pipes, as mentioned earlier at the beginning of Section 3. The present fracture mechanics approach can be used to rank fracture resistance of different materials with an enormously reduced effort. 6. Prediction of pipes lifetime Eq. (3) can be used as the basis of a simple analytical model able to predict lifetime of polymeric pipes; in the present study the contribution of initiation time to the total failure time was neglected, as previously done in [10]. This is only a rst approximation giving conservative predictions that were compared against experimental data obtained from full-scale tests on pipes. In order to apply the model one needs to properly dene the geometry of both the pipe and the initial defect, and use a suitable shape factor; relevant material parameters (namely A and q) need to be known as well. A pipe geometry analogous to that sketched in Fig. 12 was considered: a semi-circular aw was assumed to be situated at the pipe inner surface, lying on a radial plane. Physical dimensions were chosen according to the actual dimensions of the pipes used by Basell for full-scale tests on i-PB; they are listed in Table 2. Experimental observations indicate that fracture always initiates at the inner surface and quality controls performed prior to pipe testing excluded the presence of defects larger than 50 lm: the location and size of the initial defect were chosen accordingly. When internal pressure is applied to a pipe pure mode I conditions are generated at the crack tip of a radial defect. The latter was assumed to propagate keeping a semi-circular shape: in this way K could be calculated as a function of the hoop stress and the defect size by using the same shape factor (taken from [20]) throughout all the analysis. Pipe lifetimes were evaluated for different levels of applied hoop stress (up to 20 MPa) by integrating Eq. (3) for a crack growing from the initial defect size a0 to the wall thickness s. The choice of which material parameters to use is not straightforward, since both materials exhibit a transition in the K vs. da/dt master curve. However, even for the highest level of applied stress (20 MPa) K values ranged from 100.66 (0.2 MPa m, for aa0) up to 100.48 ((3.0 MPa m, when as). By looking at Fig. 10 it is obvious that in these conditions K values lie in the stable propagation region for most of the pipe life. Therefore, predictions were made considering A and q as obtained from the stable part of each of the two master curves at 23 C, thus extrapolating the stable behaviour to the whole K range. Experimental data from full-scale tests on pipes performed by Basell were available at 23, 70 and 95 C and the same temperatures were considered in the model. The shift factor shown in Fig. 11 was used to obtain the K vs. da/dt curve at 70 C; the curve at 95 C was generated by applying a shift factor obtained by linear extrapolation. A comparison between model predictions and full-scale experiments is shown in Fig. 13. The FM model predictions are shown as the lines on the right and they should represent the region of brittle failure for the two materials. However, in the time-scale considered most of the experimental pipe failures were reported as being ductile. Actually a fair estimate of the failure time in this region can be obtained by simply considering time to yield data for each stress level and temperature. Time to yield was calculated from yield stress vs. time curves reported in [10].

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Fig. 12. Cracked pipe model considered for the prediction of pipe lifetimes.

23C 70C 10 95C

stress (MPa)

1
0

experiment PB2 experiment PB1

model PB2 model PB1

10

10

10

10

10

10

10

10

10

10

time (h)
Fig. 13. Comparison between model predictions and experimental data from full-scale tests on pipes at 23, 70 and 95 C.

Only a few pipes corresponding to data points at the highest failure times (greater than 104 h) presented a failure mechanism which was reported as mixed, indicating a transition towards the brittle region; the experimental curves show a hint of a knee for these data. This is where the curves describing the brittle region are expected to intersect those for ductile

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failure and indeed this is what happens for model predictions at 23 and 70 C, with remarkably good agreement. At 95 C predicted curves seem to slightly overestimate lifetimes for both materials, nevertheless the overall agreement is substantially good and shows that this approach can be used to obtain reliable estimates of pipe lifetimes. Moreover, the model correctly reproduces the different behaviour of PB1 and PB2, with curves of the latter slightly above those of the less resistant material as it is observed on full-scale tests. It may be surprising that such a good agreement has been obtained despite neglecting initiation times: this should lead to conservative estimates of pipe lifetimes. However the model predictions strongly depend on the initial aw size. A different value of this parameter would cause an horizontal shift of the predicted curves, as discussed in [10]. This research is continuing with the aim of studying crack initiation for these materials and future developments of the model will take it into account as well.

7. Conclusions Fracture properties of two pipe grades of polybutene have been studied performing experiments on DCB and SENB congurations. The existence of two mechanisms of stable and partially unstable crack propagation has been observed, as previously reported in [7]. The effect of testing speed and temperature on crack stability has been investigated and a transition from stable to partially unstable crack propagation has been detected on both materials. It has been found that higher testing speeds and lower temperatures promote the occurrence of instabilities. The combined effect of testing speed and temperature ts well into a timetemperature superposition scheme and crack propagation master curves could be obtained for both materials. The two curves are characterised by a bilinear trend with a knee separating the two regions of stable and partially unstable crack propagation. The analysis performed using the fracture mechanics approach gave two main results: 1. Direct comparison of the crack propagation master curves can in most cases (unless they intersect) give a ranking of different materials with respect to their creep crack growth resistance. In the present case the more crystalline grades curve lies above the other materials, thus indicating a slower crack speed for any value of the applied stress. 2. Quantitative predictions of manufactured items lifetime may be obtained by using crack propagation data in conjunction with simple models based on FM and the different performance of the materials investigated has been evaluated. The analysis and the predictions agree well with experimental data obtained by the materials supplier from full-scale test on pipes. Fracture mechanics therefore can be used to perform accelerated testing and proves itself to be a quick, inexpensive and reliable method to evaluate the long-term performance of different materials.

Acknowledgements The authors wish to thanking Evaristo Odinol for his precious support in performing DCB tests and analysing the data and Mr. Oscar Bressan for the specimen preparation.

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